[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

JPH11279710A - Bearing steel excellent in acoustic property and quietness - Google Patents

Bearing steel excellent in acoustic property and quietness

Info

Publication number
JPH11279710A
JPH11279710A JP10003198A JP10003198A JPH11279710A JP H11279710 A JPH11279710 A JP H11279710A JP 10003198 A JP10003198 A JP 10003198A JP 10003198 A JP10003198 A JP 10003198A JP H11279710 A JPH11279710 A JP H11279710A
Authority
JP
Japan
Prior art keywords
content
less
steel
acid
quietness
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP10003198A
Other languages
Japanese (ja)
Inventor
Yukitaka Mizuno
幸隆 水野
Sadayoshi Furusawa
貞良 古澤
Koji Kanatsuki
宏治 金築
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Koshuha Steel Co Ltd
Kobe Steel Ltd
Original Assignee
Nippon Koshuha Steel Co Ltd
Kobe Steel Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nippon Koshuha Steel Co Ltd, Kobe Steel Ltd filed Critical Nippon Koshuha Steel Co Ltd
Priority to JP10003198A priority Critical patent/JPH11279710A/en
Publication of JPH11279710A publication Critical patent/JPH11279710A/en
Pending legal-status Critical Current

Links

Landscapes

  • Rolling Contact Bearings (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain a steel excellent in an acoustic property and quietness by making an acid insoluble impurity less than a specified pieces per unit steel when dissolving, in a mixed acid aqueous solution heated to a specified temp, the steel which contains a specified content in each of C, Si, Mn, Cr, Al and the balance Fe with inevitable impurities, and restricts Ti, O in the impurities to a specified content. SOLUTION: A content, by weight, is 0.6-1.2% C, 0.1-2.0% Si, 0.1-2.0% Mn, 10.0-14.0% Cr, <=0.04% Al. Ti, O in the impurities, by weight, <=0.0015% T, <=0.0012% O. A mixed acid aqueous solution is prepared by mixing, by mass, 60% nitric acid, 96% sulfuric acid, pure water in the volume ratio of 25:1:55 and heating to 90-95 deg.C. An acid insuluble impurity includes Al2 O3 of 50%, and its size is >=15 μm major diameter and is less than 19 pieces in 10 g of the steel. In the case corrosion resistance is not required, a Cr content is 0.8-2.0%, and in the case of needing that of medium degree, it is 2.0-10.0%.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、ころ軸受や玉軸受
のような転がり軸受に使用する軸受材料、特にエアコ
ン,コンピュータのディスクドライブ,ビデオおよびオ
ーディオ機器等、音響特性,静粛性が要求される精密機
器に使用して最適な軸受用鋼に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention requires a bearing material used for a rolling bearing such as a roller bearing or a ball bearing, particularly an air conditioner, a disk drive of a computer, a video and audio equipment, etc., which require acoustic characteristics and quietness. It relates to the most suitable bearing steel for use in precision equipment.

【0002】[0002]

【従来の技術】ここで音響特性,静粛性とは、転がり軸
受その他の転動装置が作動中に発生する振動により生じ
る騒音の少なさを指すもので、工作機械や建設機械など
ではそれほど問題にならないが、例えばHDDやVTR
等のような振動を極度に嫌う精密機器に使用される比較
的小型の玉軸受などにおいては、音響特性,静粛性が大
きな問題となってくる。これら小型の玉軸受では、負荷
荷重がさほど大きくないために転動疲労寿命などの疲労
特性はあまり問題視されず、回転時の静粛性,音響特性
が重要視され、従来から研究,開発は種々なされてい
る。
2. Description of the Related Art The term "acoustic characteristics and quietness" as used herein refers to a level of noise generated by vibrations generated during the operation of rolling bearings and other rolling devices, and is a serious problem in machine tools and construction machines. No, for example, HDD or VTR
In relatively small ball bearings and the like used in precision equipment that extremely dislikes vibrations, acoustic characteristics and quietness are serious problems. In these small ball bearings, since the applied load is not so large, fatigue characteristics such as rolling fatigue life are not regarded as much problems, and quietness and acoustic characteristics during rotation are regarded as important. It has been done.

【0003】ところで、軸受用鋼の音響特性,静粛性で
注目されるのは、使用初期の音響特性と、使用中の経年
変化による音響特性の劣化の2種類である。まず使用初
期の音響特性であるが、これは軸受部品の形状的な仕上
げ精度に大きく左右される。そして材料面で、この仕上
げ精度を大きく左右するのは基地と硬さの大きく異なっ
た非金属介在物や共晶炭化物の数と大きさである。ま
た、使用中の経年変化による音響特性については、使用
初期の音響特性に問題の無いレベルであっても、軸受部
品使用中において基地と硬質な非金属介在物や共晶炭化
物との間に生じる摩耗差が表面形状,表面粗さ等の精度
劣化をまねき、使用中の音響特性を低下させる。このう
ち共晶炭化物については特開昭61−163244号公
報にその大きさと量の限界について開示されている。
[0003] By the way, two types of attention are paid to the acoustic characteristics and quietness of the bearing steel: an acoustic characteristic at the beginning of use and deterioration of the acoustic characteristics due to aging during use. First, the acoustic characteristics in the initial stage of use largely depend on the finishing accuracy of the shape of the bearing component. In terms of material, the finishing accuracy is greatly affected by the number and size of non-metallic inclusions and eutectic carbides whose hardness differs greatly from that of the matrix. In addition, as for the acoustic characteristics due to aging during use, even when the acoustic characteristics in the initial stage of use have no problem, they occur between the base and hard nonmetallic inclusions or eutectic carbides during use of the bearing parts. The difference in wear leads to deterioration of accuracy such as surface shape and surface roughness, and lowers acoustic characteristics during use. Among them, the eutectic carbides are disclosed in Japanese Patent Application Laid-Open No. 61-163244 with respect to the size and amount limits.

【0004】一方、非金属介在物は軸受部品の諸特性
(例えば、転動疲労寿命)にとって有害であることは一
般的に知られており、この非金属介在物低減のために
O,Tiなどを低く制御したものは多く開示されてい
る。非金属介在物を低減するための手段としてO,Ti
などを低く制御するようにした従来公知のものは、軸受
或いは転動部品の転動疲労寿命に着目してなされたもの
であり、静粛性,音響特性に着目して非金属介在物の大
きさ,数,存在確率等に関して研究されたものではな
い。したがって、静粛性,音響特性と非金属介在物の大
きさ,数等との関係は何ら明らかにされていない。
[0004] On the other hand, it is generally known that nonmetallic inclusions are harmful to various characteristics (for example, rolling fatigue life) of bearing parts. Many have been disclosed in which is controlled low. As a means for reducing non-metallic inclusions, O, Ti
In the prior art, which is controlled to be low, focusing on the rolling fatigue life of a bearing or a rolling part, and focusing on quietness and acoustic characteristics, the size of nonmetallic inclusions is reduced. It has not been studied in terms of number, number, existence probability, etc. Therefore, the relationship between quietness and acoustic characteristics and the size and number of nonmetallic inclusions has not been clarified at all.

【0005】[0005]

【発明が解決しようとする課題】前記特開昭61−16
3244号公報には、軸受部品の形状的な仕上げ精度を
大きく左右する共晶炭化物の大きさと量の限界について
開示されているが、C及びCrの成分範囲が重量%で、
C:0.6〜1.2%、Cr:0.8〜14.0%のも
のにあっては、鋼塊の大きさの制御、ソーキングを実施
する等の製造方法の発達により共晶炭化物が音響特性に
及ぼす影響は比較的少なくなっている。加えて、非金属
介在物の数と大きさに着目したものではなかった。
SUMMARY OF THE INVENTION The above-mentioned Japanese Patent Application Laid-Open No. 61-16 / 1986
Japanese Unexamined Patent Publication No. 3244 discloses a limit on the size and amount of eutectic carbide which greatly affects the finishing accuracy of the shape of a bearing component.
In the case of C: 0.6 to 1.2% and Cr: 0.8 to 14.0%, eutectic carbides are developed due to the development of manufacturing methods such as controlling the size of the steel ingot and performing soaking. Has a relatively small effect on the acoustic characteristics. In addition, it did not focus on the number and size of nonmetallic inclusions.

【0006】軸受部品の形状的な仕上げ精度により大き
く影響するのは、この発明では着目していない非金属介
在物の数と大きさ、すなわち共晶炭化物に比較して大き
く、数が多く、製造工程において制御の難しいAl2
3 含有率50%以上の硬質の酸化物系介在物の大きさと
数である。
[0006] The shape finishing accuracy of the bearing component greatly affects the number and size of the non-metallic inclusions which are not considered in the present invention, that is, the number and size of the non-metallic inclusions are large and large as compared with the eutectic carbide, and the number of the non-metallic inclusions is large in the manufacturing process. Al 2 O difficult to control
3 The size and number of hard oxide-based inclusions having a content of 50% or more.

【0007】Al2 3 含有率50%以上の硬質の酸化
物系介在物で、粗大なものが多数存在するような軸受用
鋼を軸受け部品の素材として使用した場合には、この粗
大で硬質な非金属介在物が転動装置部品の表面に出現
し、仕上加工精度を悪化させて音響特性を悪くする。
又、使用中において基地と硬質な非金属介在物との間に
生じる摩耗差が表面形状の精度劣化をまねき、経年変化
による音響特性の劣化を引き起こす。逆に、硬質の酸化
物系介在物の大きさと数、存在比を的確に把握してコン
トロールすることにより、使用初期の音響特性を向上さ
せることができることを本発明者等は知得した。
[0007] When a bearing oxide steel containing a large number of hard oxide inclusions having an Al 2 O 3 content of 50% or more is used as a material for a bearing component, the coarse and hard steel is used. Non-metallic inclusions appear on the surface of the rolling device component, deteriorating the finishing accuracy and deteriorating the acoustic characteristics.
In addition, a difference in abrasion generated between the base and the hard nonmetallic inclusion during use causes deterioration in accuracy of the surface shape, and causes deterioration in acoustic characteristics due to aging. On the contrary, the present inventors have found that the acoustic characteristics at the beginning of use can be improved by accurately grasping and controlling the size, number, and abundance ratio of the hard oxide-based inclusions.

【0008】本発明は、上記のような従来の諸事情に着
目して成されたものであり、音響特性,静粛性に悪影響
を及ぼす硬質の酸化物系非金属介在物を正確且つ定量的
に把握する方法を用いてその数と大きさを制御し、ひい
ては優れた音響特性,静粛性を安定して得られる軸受用
鋼を提供することを目的としたものである。
The present invention has been made in view of the above-mentioned conventional circumstances, and is capable of accurately and quantitatively detecting hard oxide-based nonmetallic inclusions that adversely affect acoustic characteristics and quietness. It is an object of the present invention to provide a bearing steel capable of controlling the number and size thereof using a grasping method, and thereby obtaining stable acoustic characteristics and quietness.

【0009】[0009]

【課題を解決するための手段】前記目的を達成すること
ができた本発明に係る音響特性,静粛性に優れた軸受用
鋼とは、重量%で、C:0.6〜1.2%、Si:0.
1〜2.0%、Mn:0.1〜2.0%、Cr:0.8
〜14.0%、Al:0.04%以下、残部がFeおよ
び不可避不純物からなり、該不可避不純物中Ti:0.
0015%以下、O:0.0012%以下にそれぞれ抑
制した鋼材であって、90〜95℃に加熱された60%
(質量%を意味する:以下同じ)の硝酸、96%の硫
酸、純水の体積比が25:1:55の混合酸水溶液に前
記鋼材を溶解させた場合に、長径15μm以上の大きさ
でAl2 3 含有率が50%以上である酸不溶性介在物
の個数が前記鋼材10g当たり10個未満であるところ
にその特徴を有している。
The bearing steel excellent in acoustic characteristics and quietness according to the present invention, which can achieve the above object, is expressed in terms of% by weight, C: 0.6 to 1.2%. , Si: 0.
1 to 2.0%, Mn: 0.1 to 2.0%, Cr: 0.8
1414.0%, Al: 0.04% or less, the balance being Fe and unavoidable impurities.
0015% or less, O: a steel material suppressed to 0.0012% or less, respectively, and 60% heated to 90 to 95 ° C.
When the steel material is dissolved in a mixed acid aqueous solution (mean% by mass: the same applies hereinafter) of nitric acid, 96% sulfuric acid, and pure water having a volume ratio of 25: 1: 55, the long diameter is 15 μm or more. This is characterized in that the number of acid-insoluble inclusions having an Al 2 O 3 content of 50% or more is less than 10 per 10 g of the steel material.

【0010】また上記鋼材において、Crは耐食性と硬
さ、コスト等を勘案すると、重量%で、10.0〜1
4.0%、2.0〜10.0%、0.8〜2.0%
の範囲に区分される。また、必要によりNi:0.1〜
2.0%、Cu:0.1〜1.0%、Mo:0.1〜
2.0%、W:0.1〜1.0%、V:0.05〜1.
0%、Nb:0.01〜1.0%から選ばれる1種また
は2種以上を含有させることによって、その性能を一段
と向上させることができる。
In the above steel material, Cr is 10.0 to 1% by weight in consideration of corrosion resistance, hardness, cost and the like.
4.0%, 2.0-10.0%, 0.8-2.0%
Are divided into ranges. If necessary, Ni: 0.1 to
2.0%, Cu: 0.1-1.0%, Mo: 0.1-
2.0%, W: 0.1-1.0%, V: 0.05-1.
By containing one or more selected from 0% and Nb: 0.01 to 1.0%, the performance can be further improved.

【0011】[0011]

【発明の実施の形態】本発明は、静粛性,音響特性に軸
受部品の素材(本発明では鋼材)側の要因として最も大
きく影響し、鋼材の製造工程において制御の難しいAl
2 3 含有率50%以上の硬質の酸化物系介在物の大き
さと数、存在比を的確に把握してコントロールした鋼材
にあり、その好ましい基本成分は以下の通りである。
BEST MODE FOR CARRYING OUT THE INVENTION The present invention has the greatest influence on the quietness and acoustic characteristics as a factor of the material (steel material in the present invention) of a bearing component, and it is difficult to control the Al in the steel material manufacturing process.
It is a steel material in which the size, number, and abundance ratio of hard oxide-based inclusions having a 2 O 3 content of 50% or more are accurately grasped and controlled, and preferred basic components are as follows.

【0012】Cの含有量は重量%(以下、同じ)で、
0.6〜1.2%とする。Cは焼入硬さを増大させ、室
温,高温における強度を維持して耐摩耗性を付与するた
めに必須の元素である。含有量が0.6%未満であると
焼入硬さが不足して耐摩耗性を維持することができな
い。一方、1.2%を越えると長時間ソーキングでも拡
散しきれない巨大な共晶炭化物が生成するため、軸受部
品の静粛性を始めとして被研削性,冷間鍛造性,被切削
性を低下させる。
The content of C is% by weight (hereinafter the same),
0.6 to 1.2%. C is an element essential for increasing quenching hardness, maintaining strength at room temperature and high temperature, and imparting wear resistance. When the content is less than 0.6%, the quenching hardness is insufficient and the wear resistance cannot be maintained. On the other hand, if it exceeds 1.2%, a giant eutectic carbide which cannot be diffused even by soaking for a long time is generated, and therefore, the grindability, cold forgeability, and machinability are reduced, including the quietness of the bearing component. .

【0013】また、Siの含有量は0.1〜2.0%と
する。このSiは製鋼工程における脱酸のために必要な
元素であり、また耐摩耗性と強度を増大する効果があ
り、少なくとも0.1%は必要である。しかし、含有量
が2.0%を越えると冷間鍛造性,被切削性を低下させ
るので0.1〜2.0%とする。
Further, the content of Si is set to 0.1 to 2.0%. This Si is an element necessary for deoxidation in the steel making process, and has an effect of increasing wear resistance and strength. At least 0.1% is necessary. However, if the content exceeds 2.0%, the cold forgeability and machinability deteriorate, so the content is set to 0.1 to 2.0%.

【0014】Mnの含有量は0.1〜2.0%とする。
このMnは焼入性を向上させて強度を増大させるが、多
すぎると残留オーステナイトを増加させて逆に強度を低
下させ、また寸法の経年劣化を引き起こす。このため成
分範囲を0.1〜2.0%とした。
[0014] The Mn content is 0.1 to 2.0%.
This Mn improves the hardenability to increase the strength, but if it is too much, it increases the retained austenite, conversely lowers the strength and causes aging of the dimensions. Therefore, the component range is set to 0.1 to 2.0%.

【0015】そして、Crの含有量は、.10.0〜
14.0%、.2.0〜10.0%、.0.8〜
2.0%の範囲に区分される。Crは特に重要な元素で
あり、強度,焼入性を向上させるとゝもに、耐食性,耐
熱性を付与する。またCrはCと結びついて微細な炭化
物を形成して耐摩耗性を付与する。しかし、Cr含有量
が0.8%未満ではその効果がなく、14.0%を越え
ると巨大な共晶炭化物が生成されるため、0.8〜1
4.0%とする。
The content of Cr is. 10.0 ~
14.0%,. 2.0-10.0%,. 0.8 ~
It is classified into the range of 2.0%. Cr is a particularly important element, and improves corrosion resistance and heat resistance while improving strength and hardenability. In addition, Cr forms fine carbides in combination with C to provide wear resistance. However, if the Cr content is less than 0.8%, the effect is not obtained. If the Cr content exceeds 14.0%, a huge eutectic carbide is generated.
4.0%.

【0016】ここで、Cr:0.8〜14.0%の範囲
では、その含有量が増大するに伴い耐食性は図1のよう
に変化する。軸受部品の場合、用途によって要求される
耐食性は大きく異なる。通常の用途で耐食性を要求され
ないような場合、Cr含有量は0.8〜2.0%で十分
であり、この場合のCrの役割は強度,焼入性の向上で
ある。しかし、十分な耐蝕性が要求される用途、例えば
HDD用の玉軸受のように組み付け時に完全に脱脂され
て以後錆を嫌うような軸受部品や、海岸地方で使用され
る可搬性の精密機器では、Crの含有量は最低でも1
0.0%必要であり、10.0〜14.0%が範囲とな
る。これらの中間の範囲2.0〜10.0%では、軸受
部品の用途ごとに必要な耐食性に応じてCr量を選択す
る。Crは多く含有すると当然製造コストは含有量に比
例して上昇するので、要求される耐食性とコストに応じ
てCrの成分範囲を選択することになる。
Here, in the range of Cr: 0.8 to 14.0%, the corrosion resistance changes as shown in FIG. 1 as its content increases. In the case of bearing components, the required corrosion resistance varies greatly depending on the application. In the case where corrosion resistance is not required in ordinary applications, the Cr content is sufficient at 0.8 to 2.0%, and the role of Cr in this case is to improve strength and hardenability. However, in applications where sufficient corrosion resistance is required, such as bearing parts that are completely degreased during assembly, such as ball bearings for HDDs, and are susceptible to rust, and portable precision equipment used in coastal areas. , Cr content is at least 1
0.0% is required, and the range is 10.0 to 14.0%. In the intermediate range of 2.0 to 10.0%, the amount of Cr is selected according to the corrosion resistance required for each use of the bearing component. If a large amount of Cr is contained, the production cost naturally increases in proportion to the content. Therefore, the range of the Cr component should be selected according to the required corrosion resistance and cost.

【0017】また、Alの含有量は、0.040%以下
とする。このAlは製鋼工程での脱酸のために必須の元
素であり、特にOを0.0012%以下にするためには
ある程度の添加は必要である。しかし多量に含有すると
硬質のAl2 3 含有量の高い酸化物系介在物を多量に
生成するため、上限を0.040%とする。
The content of Al is set to 0.040% or less. This Al is an indispensable element for deoxidation in the steel making process, and in particular, a certain amount of addition is necessary to reduce O to 0.0012% or less. However, if contained in a large amount, a large amount of hard oxide-based inclusions having a high Al 2 O 3 content is generated, so the upper limit is made 0.040%.

【0018】以上が本発明に係る鋼材の基本成分である
が、つぎに不可避不純物の内Ti,Oを下記のように限
定する。すなわち、Tiの含有量は0.0015%以下
とする。このTiは硬質の非金属介在物TiNを形成し
て静粛性,音響特性を劣化させるので低いことが望まし
いが、0.0015%までは許容される。したがって上
限を0.0015%とする。
The above are the basic components of the steel material according to the present invention. Next, Ti and O among the inevitable impurities will be limited as follows. That is, the content of Ti is set to 0.0015% or less. This Ti is preferably low because it forms hard non-metallic inclusions TiN and degrades quietness and acoustic characteristics, but it is allowable up to 0.0015%. Therefore, the upper limit is made 0.0015%.

【0019】また、Oの含有量を0.0012%以下と
する。Oは硬質の酸化物系非金属介在物を形成して静粛
性,音響特性を劣化させるので低いことが望ましいが、
0.0012%までは許容される。よって、上限を0.
0012%とする。しかし、前述のように、Oの含有量
が0.0012%以下ではO量と酸化物系介在物の個数
には明確な相関は認められない。したがって、静粛性,
音響特性に有害な長径15μm以上で、Al2 3 含有
率50%以上の硬質の酸化物系非金属介在物の個数を最
適な測定方法を指定して別に規定する。
The content of O is set to 0.0012% or less. O is preferably low because it forms hard oxide-based nonmetallic inclusions and degrades quietness and acoustic characteristics.
Up to 0.0012% is acceptable. Therefore, the upper limit is set to 0.
0012%. However, as described above, when the O content is 0.0012% or less, no clear correlation is observed between the O content and the number of oxide-based inclusions. Therefore, quietness,
The number of hard oxide-based nonmetallic inclusions having a major axis of 15 μm or more harmful to acoustic characteristics and an Al 2 O 3 content of 50% or more is separately specified by designating an optimum measurement method.

【0020】ここで、O,Ti量と非金属介在物の数,
大きさとの関係について述べると、Tiは生成する介在
物がTiNにほぼ限定されるので比較的単純な関係で整
理され、Ti量とTi系非金属介在物の数,大きさとは
ある程度の相関が認められ、Tiの分析値から非金属介
在物の推定はある程度可能である。これに対して、Oは
Al,Si,Ca,Mg,Mn等と結びついて多種類の
非金属介在物を生成するうえに、酸化物系介在物にはス
ラグの巻き込み、製鋼工程で溶損した耐火物の混入など
が含まれる。
Here, the amounts of O and Ti, the number of nonmetallic inclusions,
Regarding the relationship with the size, the inclusions of Ti are arranged in a relatively simple relationship since the generated inclusions are almost limited to TiN, and there is a certain correlation between the amount of Ti and the number and size of the Ti-based nonmetallic inclusions. , Ti can be estimated to some extent from the analysis values of Ti. On the other hand, O combines with Al, Si, Ca, Mg, Mn, etc. to generate various kinds of nonmetallic inclusions, and slag is involved in oxide-based inclusions, and is melted in the steel making process. Includes refractories.

【0021】そのために、O量が0.0012%以下の
清浄度の高い鋼では、O量と非金属介在物の数,大きさ
との間にはほとんど相関がない。このことは、文献(材
料とプロセス,4(1991),1178や材料とプロセス,
4(1991),321 )でも開示されている。したがって、軸
受用鋼中の非金属介在物の評価方法は直接的にその数と
大きさを最適な方法で測定するしかない。
Therefore, in a highly clean steel having an O content of 0.0012% or less, there is almost no correlation between the O content and the number and size of nonmetallic inclusions. This has been described in the literature (Materials and Processes, 4 (1991), 1178, Materials and Processes,
4 (1991), 321). Therefore, the only method of evaluating nonmetallic inclusions in bearing steel is to directly measure the number and size of the nonmetallic inclusions using an optimal method.

【0022】従来から行われている非金属介在物の測定
方法は、鋼材のL断面(長手方向縦断面)を顕微鏡観察
し、該断面に存在する介在物の数や大きさ、長さを調べ
る方法が一般的であり、この方法はJIS G 055
5やASTM E−45にも規定されている。しかし、
鋼材のL断面観察はごく限られた1断面に存在する介在
物を対象とする評価であり、加えて、鋼材の断面におけ
る観察では、個々の非金属介在物の最大径を測定する確
率は極めて小さいため、限られた面積での観察では精度
の良い評価は困難である。
Conventional methods for measuring non-metallic inclusions include a method of observing the L section (longitudinal longitudinal section) of a steel material with a microscope and examining the number, size, and length of inclusions present in the section. This method is generally used and is described in JIS G 055.
5 and ASTM E-45. But,
The observation of the L cross section of a steel material is an evaluation of inclusions existing in only a limited cross section. In addition, in the observation of a cross section of a steel material, the probability of measuring the maximum diameter of each nonmetallic inclusion is extremely high. Due to the small size, it is difficult to perform accurate evaluation in observation with a limited area.

【0023】特に、O量が0.0012%以下では酸化
物系非金属介在物の存在確率が減少するために鋼材の断
面観察では精度に限界がある。また、多くの種類の酸化
物系非金属介在物の中で有害なAl2 3 の含有率50
%以上の硬質の介在物を見分けるのも困難であった。こ
こで、特開平3−126839号公報には、軸受用鋼の
介在物を電子ビーム溶解抽出評価法によって保証するこ
とが開示されている。しかし、これは転動疲労寿命に着
目して非金属介在物を測定したものであり、静粛性,音
響特性との関係を調べたものではない。この電子ビーム
溶解抽出評価法は、電子ビームによりサンプルを溶融し
比重の軽い非金属介在物を浮上させるものである。
In particular, when the O content is 0.0012% or less, the accuracy of observation of a cross section of a steel material is limited because the existence probability of oxide-based nonmetallic inclusions decreases. In addition, a harmful Al 2 O 3 content of 50% among many kinds of oxide-based nonmetallic inclusions.
% Of hard inclusions was difficult to identify. Here, Japanese Unexamined Patent Publication (Kokai) No. 3-126839 discloses that inclusions in bearing steel are guaranteed by an electron beam melting and extraction evaluation method. However, this is a measurement of nonmetallic inclusions with a focus on rolling fatigue life, and does not examine the relationship between quietness and acoustic characteristics. In this electron beam melting and extraction evaluation method, a sample is melted by an electron beam to float nonmetallic inclusions having a low specific gravity.

【0024】したがって、この電子ビーム溶解抽出評価
法にあってはサンプルを完全に溶解せねばならず、低融
点の(鋼材の融点に近い融点を持つ)非金属介在物にあ
っては再溶解してしまうので測定できない。また再溶解
しない非金属介在物であっても高温のため原形を保った
まま完全に浮上させることは困難であり、凝集,焼結で
より大きなサイズで観察されてしまう可能性が高く、精
度の高い測定は困難であった。
Therefore, in this electron beam dissolution extraction evaluation method, the sample must be completely dissolved, and in the case of non-metallic inclusions having a low melting point (having a melting point close to the melting point of steel), the sample must be completely dissolved. Measurement is impossible. Even non-metallic inclusions that do not re-dissolve are difficult to completely float while maintaining their original shape due to high temperatures, and are likely to be observed in larger sizes due to aggregation and sintering. High measurements were difficult.

【0025】そこで、本発明における非金属介在物の測
定では、90〜95℃に加熱された60%(質量%を意
味する:以下同じ)の硝酸、96%の硫酸、純水の体積
比が25:1:55の混合酸水溶液に鋼材を溶解させ、
酸不溶性介在物をEPMA分析を行ってAl2 3
度,長径と個数を測定する方法を採用することにより、
図2に示すような実験データを得ることができた。
Therefore, in the measurement of nonmetallic inclusions in the present invention, the volume ratio of 60% (mean% by mass; the same applies hereinafter) nitric acid, 96% sulfuric acid, and pure water heated to 90 to 95 ° C. A steel material is dissolved in a 25: 1: 55 mixed acid aqueous solution,
By adopting a method in which acid-insoluble inclusions are subjected to EPMA analysis to measure the Al 2 O 3 concentration, major axis and number thereof,
Experimental data as shown in FIG. 2 could be obtained.

【0026】本発明に係る鋼材は、さらに必要により下
記の成分元素を含有することが可能である。すなわち、
Niの含有量は0.1〜2.0%とする。このNiは本
発明において必要に応じて添加する。0.1%以上添加
すると焼入性を向上させて焼入効果深さを深くするとゝ
もに、靭性,延性を改善する効果がある。多量に含有す
ると残留オーステナイトを増加させて、軸受部品の使用
中の経年変化を引き起こし、音響特性を劣化させるの
で、上限を2.0%とする。
The steel material according to the present invention can further contain the following component elements, if necessary. That is,
The content of Ni is set to 0.1 to 2.0%. This Ni is added as needed in the present invention. Addition of 0.1% or more has the effect of improving the hardenability and increasing the hardening effect depth, and at the same time, has the effect of improving the toughness and ductility. If contained in a large amount, the retained austenite increases, causing aging during the use of the bearing component and deteriorating the acoustic characteristics. Therefore, the upper limit is made 2.0%.

【0027】Cuの含有量は0.1〜1.0%とする。
Cuは本発明において必要に応じて添加する。0.1%
以上添加すると焼入性,耐食性を向上させる。多量に含
有すると赤熱脆性を助長して熱間加工性を劣化するので
上限を1.0%とする。またMoの含有量は0.1〜
2.0%とする。このMoは本発明において必要に応じ
て添加する。0.1%以上添加すると焼入性を向上させ
るとともに耐食性,耐摩耗性を向上させる。2.0%以
上添加するとM6 C炭化物を多量に生成し、添加効果が
飽和するとともに、静粛性,音響特性を劣化させるため
に上限を2.0%とする。
The content of Cu is 0.1 to 1.0%.
Cu is added as necessary in the present invention. 0.1%
Addition of the above improves hardenability and corrosion resistance. If it is contained in a large amount, red hot brittleness is promoted and hot workability is deteriorated, so the upper limit is made 1.0%. The content of Mo is 0.1 to
2.0%. This Mo is added as needed in the present invention. Addition of 0.1% or more improves hardenability and corrosion resistance and wear resistance. When added in an amount of 2.0% or more, a large amount of M 6 C carbides is generated, the effect of addition is saturated, and the upper limit is set to 2.0% in order to degrade quietness and acoustic characteristics.

【0028】Wの含有量は0.1〜1.0%とする。こ
のWは本発明において必要に応じて添加する。その効果
はMoと同様である。1.0%で効果が飽和するので、
上限を1.0%とする。そして、Vの含有量は0.05
〜1.0%とする。Vは本発明において必要に応じて添
加する。0.05%以上添加すると微細なVC炭化物を
生成し、結晶粒径を微細化すると共に耐摩耗性と耐熱性
を向上させる。しかし1.0%以上添加するとVC炭化
物が粗大化し、静粛性,音響特性を劣化させるので上限
を1.0%とする。
The content of W is 0.1-1.0%. This W is added as needed in the present invention. The effect is the same as Mo. Since the effect is saturated at 1.0%,
The upper limit is set to 1.0%. And the content of V is 0.05
To 1.0%. V is added as needed in the present invention. When added in an amount of 0.05% or more, fine VC carbides are formed, and the crystal grain size is reduced, and the wear resistance and heat resistance are improved. However, if added in an amount of 1.0% or more, the VC carbides become coarse and the quietness and acoustic characteristics deteriorate, so the upper limit is made 1.0%.

【0029】またNbの含有量は0.01〜1.0%と
する。Nbは本発明において必要に応じて添加する。
0.01%以上の添加で微細なNbC炭化物を生成して
結晶粒径を微細化する。1.0%以上添加するとNbC
炭化物が粗大化して静粛性,音響特性を劣化させるので
上限を1.0%とする。
The content of Nb is 0.01 to 1.0%. Nb is added as needed in the present invention.
By adding 0.01% or more, fine NbC carbides are generated to refine the crystal grain size. If more than 1.0% is added, NbC
The upper limit is set to 1.0% because carbides are coarsened and the silence and acoustic characteristics are deteriorated.

【0030】[0030]

【実施例】次に、本発明を実施例及び比較例により具体
的に説明するために、表1に本発明鋼材および比較鋼材
の化学組成を示す。供試した鋼材は、溶鋼を精錬,脱ガ
ス処理した後に造塊し、熱間圧延でφ25mmの棒材と
φ5.5mmの線材としたものである。この表1中N
0.1〜N0.19は本発明鋼材であり、N0.20〜
N0.24は従来鋼材である。
EXAMPLES Next, in order to specifically explain the present invention with reference to Examples and Comparative Examples, Table 1 shows the chemical compositions of the steel materials of the present invention and comparative steel materials. The steel material tested was obtained by subjecting molten steel to refining and degassing, and then forming an ingot, followed by hot rolling into a rod having a diameter of 25 mm and a wire having a diameter of 5.5 mm. N in Table 1
0.1 to N0.19 are steel materials of the present invention, and N0.20 to N0.19.
N0.24 is a conventional steel material.

【0031】[0031]

【表1】[Table 1]

【0032】表2に、本発明鋼材および比較鋼材につい
ての材料中の酸不溶性介在物の測定結果と、熱処理条
件、熱処理後の諸特性を示す。酸不溶性介在物の測定
は、線材の表面スケールを除去後、90〜95℃に加熱
された60%(質量%を意味する:以下同じ)の硝酸、
96%の硫酸、純水の体積比が25:1:55の混合酸
水溶液で前記供試鋼材を溶解した。
Table 2 shows the measurement results of the acid-insoluble inclusions in the steel material of the present invention and the comparative steel material, heat treatment conditions, and various properties after the heat treatment. The measurement of the acid-insoluble inclusions is performed by removing the surface scale of the wire, heating 60% to 90 ° C to 95 ° C (mean% by mass: the same applies hereinafter) nitric acid,
The test steel was dissolved in a mixed acid aqueous solution of 96% sulfuric acid and pure water at a volume ratio of 25: 1: 55.

【0033】[0033]

【表2】[Table 2]

【0034】鋼材を溶解した後、篩い目5μmのフィル
タで吸引濾過し、次に篩い目1μmのフィルタを用い
て、純水,希塩酸,エタノールで洗浄した。洗浄後、酸
不溶性介在物を採取したフィルタを乾燥し、EPMAで
フィルタ上の非金属介在物の分析を行い、Al2 3
度,長径と個数を測定した。その測定値をグラフにあら
わしたものが図2である。
After dissolving the steel material, it was subjected to suction filtration with a filter having a sieve of 5 μm, and then washed with pure water, dilute hydrochloric acid and ethanol using a filter having a sieve of 1 μm. After washing, the filter from which the acid-insoluble inclusions were collected was dried, and non-metallic inclusions on the filter were analyzed by EPMA, and the Al 2 O 3 concentration, major axis, and number were measured. FIG. 2 shows the measured values in a graph.

【0035】また、共晶炭化物は、光学顕微鏡にて鋼材
のL断面(長手方向縦断面)を330mm2 観察し、長
径15μm以上のものが存在するかどうかを確認した。
そしてまた、耐食性に関しては、純水噴霧試験を200
Hrと5%NaClの塩水噴霧試験を3Hr実施して、
目視による1〜5点の5段階評価を行った。その測定値
をグラフにあらわしたものが図1である。なお、点数は
5点が最も良い。
As for the eutectic carbide, the L section (longitudinal section in the longitudinal direction) of the steel material was observed with an optical microscope at 330 mm 2 , and it was confirmed whether or not there was one having a major axis of 15 μm or more.
As for the corrosion resistance, a pure water spray test was conducted for 200 hours.
The salt spray test of Hr and 5% NaCl was performed for 3 hours,
Five-stage evaluation of 1 to 5 points was visually performed. FIG. 1 shows the measured values in a graph. The best score is 5 points.

【0036】さらに静粛性,音響特性に関しては、供試
材で玉軸受の内輪と外輪を作製し、SUJ2製のボール
を組み込んでAFBMA(The Anti-Friction Bearing M
anufacturers Association, Inc.) の規格に準拠して行
ったアンデロン値を中周波数帯域(300〜1800H
z)、高周波数帯域(1800〜10000Hz)につ
いて夫々測定した。なお、表2に示す数値は、試料N
0.20(従来鋼)を基準(100)とした指数で表示
した。
Further, regarding the quietness and acoustic characteristics, the inner and outer rings of the ball bearing were manufactured from the test materials, and the balls made of SUJ2 were incorporated into the AFBMA (The Anti-Friction Bearing M).
anderon values measured in accordance with the standards of the Anufacturers Association, Inc.
z) and a high frequency band (1800 to 10000 Hz). The values shown in Table 2 correspond to the values of sample N
It was indicated by an index using 0.20 (conventional steel) as a reference (100).

【0037】本発明鋼材の数値は、中周波数帯域及び高
周波数帯域とも従来鋼材の数値より小さく、静粛性に優
れていることが判る。なお、図3は本発明鋼材の表2に
示す非金属介在物の個数と静粛性の指数を表した図であ
る。
The numerical value of the steel material of the present invention is smaller than that of the conventional steel material in both the middle frequency band and the high frequency band, indicating that the steel material is excellent in quietness. FIG. 3 is a diagram showing the number of nonmetallic inclusions and an index of quietness shown in Table 2 of the steel material of the present invention.

【0038】[0038]

【発明の効果】本発明に係る軸受用鋼は、上記のよう
に、鋼材の製造工程において制御の難しいAl2 3
有率50%以上の硬質の酸化物系介在物の大きさと数,
存在数を的確に把握してコントロールした構成のもので
あるから、静粛性,音響特性を安定して良好なレベルに
することができ、精密機器によって重要な問題となって
いる静粛性,音響特性に優れた小型の転がり軸受を提供
することができる、といった効果がある。
As described above, the bearing steel according to the present invention is characterized in that the size and number of hard oxide-based inclusions having an Al 2 O 3 content of 50% or more, which are difficult to control in the steel material manufacturing process,
Because it is a configuration in which the number of existence is accurately grasped and controlled, silence and acoustic characteristics can be stably set to a good level, and silence and acoustic characteristics that are important issues with precision equipment In addition, there is an effect that a small-sized rolling bearing having excellent characteristics can be provided.

【図面の簡単な説明】[Brief description of the drawings]

【図1】Cr含有量と耐食性の関係を示す図である。FIG. 1 is a diagram showing the relationship between Cr content and corrosion resistance.

【図2】O量とAl2 3 含有率50%以上の酸不溶性
介在物個数の関係を示す図である。
FIG. 2 is a graph showing the relationship between the amount of O and the number of acid-insoluble inclusions having an Al 2 O 3 content of 50% or more.

【図3】Al2 3 含有率50%以上の酸不溶性介在物
個数と静粛性指数の関係を示す図である。
FIG. 3 is a graph showing a relationship between the number of acid-insoluble inclusions having an Al 2 O 3 content of 50% or more and a quietness index.

【表1】 [Table 1]

【表2】 [Table 2]

───────────────────────────────────────────────────── フロントページの続き (72)発明者 金築 宏治 兵庫県加古川市金沢町1 株式会社神戸製 鋼所加古川製鉄所内 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Koji Kaneki 1 Kanazawacho, Kakogawa-shi, Hyogo Kobe Steel Works Kakogawa Works

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】 重量%で、C:0.6〜1.2%、S
i:0.1〜2.0%、Mn:0.1〜2.0%、C
r:10.0〜14.0%、Al:0.04%以下、残
部がFeおよび不可避不純物からなり、該不可避不純物
中Ti:0.0015%以下、O:0.0012%以下
にそれぞれ抑制した鋼材であって、90〜95℃に加熱
された60%(質量%を意味する:以下同じ)の硝酸、
96%の硫酸、純水の体積比が25:1:55の混合酸
水溶液に前記鋼材を溶解させた場合に、長径15μm以
上の大きさでAl2 3 含有率が50%以上である酸不
溶性介在物の個数が前記鋼材10g当たり10個未満で
あることを特徴とする音響特性,静粛性に優れた軸受用
鋼。
1. C .: 0.6 to 1.2% by weight, S
i: 0.1 to 2.0%, Mn: 0.1 to 2.0%, C
r: 10.0 to 14.0%, Al: 0.04% or less, balance consists of Fe and unavoidable impurities. Ti: 0.0015% or less and O: 0.0012% or less in the inevitable impurities. A 60% (mean% by mass: the same applies hereinafter) nitric acid heated to 90 to 95 ° C.,
When the steel material is dissolved in a mixed acid aqueous solution of 96% sulfuric acid and pure water having a volume ratio of 25: 1: 55, an acid having a major axis of 15 μm or more and an Al 2 O 3 content of 50% or more is used. A bearing steel having excellent acoustic characteristics and quietness, characterized in that the number of insoluble inclusions is less than 10 per 10 g of the steel material.
【請求項2】 重量%で、C:0.6〜1.2%、S
i:0.1〜2.0%、Mn:0.1〜2.0%、C
r:2.0〜10.0%、Al:0.04%以下、残部
がFeおよび不可避不純物からなり、該不可避不純物中
Ti:0.0015%以下、O:0.0012%以下に
それぞれ抑制した鋼材であって、90〜95℃に加熱さ
れた60%(質量%を意味する:以下同じ)の硝酸、9
6%の硫酸、純水の体積比が25:1:55の混合酸水
溶液に前記鋼材を溶解させた場合に、長径15μm以上
の大きさでAl2 3 含有率が50%以上である酸不溶
性介在物の個数が前記鋼材10g当たり10個未満であ
ることを特徴とする音響特性,静粛性に優れた軸受用
鋼。
2. C: 0.6 to 1.2% by weight, S
i: 0.1 to 2.0%, Mn: 0.1 to 2.0%, C
r: 2.0 to 10.0%, Al: 0.04% or less, the balance is composed of Fe and unavoidable impurities, and Ti is 0.0015% or less and O: 0.0012% or less in the unavoidable impurities. Of 60% (mean% by mass; the same applies hereinafter) nitric acid heated to 90 to 95 ° C., 9
When the steel material is dissolved in a mixed acid aqueous solution of 6% sulfuric acid and pure water having a volume ratio of 25: 1: 55, an acid having a major axis of 15 μm or more and an Al 2 O 3 content of 50% or more is used. A bearing steel having excellent acoustic characteristics and quietness, characterized in that the number of insoluble inclusions is less than 10 per 10 g of the steel material.
【請求項3】 重量%で、C:0.6〜1.2%、S
i:0.1〜2.0%、Mn:0.1〜2.0%、C
r:0.8〜2.0%、Al:0.04%以下、残部が
Feおよび不可避不純物からなり、該不可避不純物中T
i:0.0015%以下、O:0.0012%以下にそ
れぞれ抑制した鋼材であって、90〜95℃に加熱され
た60%(質量%を意味する:以下同じ)の硝酸、96
%の硫酸、純水の体積比が25:1:55の混合酸水溶
液に前記鋼材を溶解させた場合に、長径15μm以上の
大きさでAl2 3 含有率が50%以上である酸不溶性
介在物の個数が前記鋼材10g当たり10個未満である
ことを特徴とする音響特性,静粛性に優れた軸受用鋼。
3. C: 0.6-1.2% by weight, S
i: 0.1 to 2.0%, Mn: 0.1 to 2.0%, C
r: 0.8 to 2.0%, Al: 0.04% or less, the balance being Fe and unavoidable impurities.
i: a steel material suppressed to 0.0015% or less and O: 0.0012% or less, and 60% (mean% by mass: the same applies hereinafter) nitric acid heated to 90 to 95 ° C., 96
% Sulfuric acid, pure water having a volume ratio of 25: 1: 55 when the steel material is dissolved in an aqueous solution of an acid, and having a major axis of 15 μm or more and an Al 2 O 3 content of 50% or more. A bearing steel having excellent acoustic characteristics and quietness, characterized in that the number of inclusions is less than 10 per 10 g of the steel material.
【請求項4】 重量%で、Ni:0.1〜2.0%、C
u:0.1〜1.0%、Mo:0.1〜2.0%、W:
0.1〜1.0%、V:0.05〜1.0%、Nb:
0.01〜1.0%のうち一種又は2種以上を含有する
鋼材であることを特徴とする請求項1,2又は3記載の
音響特性,静粛性に優れた軸受用鋼。
4. Ni: 0.1 to 2.0% by weight, C:
u: 0.1 to 1.0%, Mo: 0.1 to 2.0%, W:
0.1-1.0%, V: 0.05-1.0%, Nb:
4. The bearing steel according to claim 1, wherein said steel is one or two or more of 0.01 to 1.0%.
JP10003198A 1998-03-27 1998-03-27 Bearing steel excellent in acoustic property and quietness Pending JPH11279710A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10003198A JPH11279710A (en) 1998-03-27 1998-03-27 Bearing steel excellent in acoustic property and quietness

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP10003198A JPH11279710A (en) 1998-03-27 1998-03-27 Bearing steel excellent in acoustic property and quietness

Publications (1)

Publication Number Publication Date
JPH11279710A true JPH11279710A (en) 1999-10-12

Family

ID=14263173

Family Applications (1)

Application Number Title Priority Date Filing Date
JP10003198A Pending JPH11279710A (en) 1998-03-27 1998-03-27 Bearing steel excellent in acoustic property and quietness

Country Status (1)

Country Link
JP (1) JPH11279710A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1158064A1 (en) * 1999-10-21 2001-11-28 Koyo Seiko Co., Ltd. Steel for large bearing and parts for large bearing
JP2003075328A (en) * 2001-09-06 2003-03-12 Koyo Seiko Co Ltd Service life estimation method for bearing steel
JP2012220015A (en) * 2011-04-14 2012-11-12 Nsk Ltd Rolling guide device
JP2014517151A (en) * 2011-05-17 2014-07-17 アクティエボラゲット・エスコーエッフ Improved bearing steel

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1158064A1 (en) * 1999-10-21 2001-11-28 Koyo Seiko Co., Ltd. Steel for large bearing and parts for large bearing
EP1158064A4 (en) * 1999-10-21 2004-09-22 Koyo Seiko Co Steel for large bearing and parts for large bearing
JP2003075328A (en) * 2001-09-06 2003-03-12 Koyo Seiko Co Ltd Service life estimation method for bearing steel
JP2012220015A (en) * 2011-04-14 2012-11-12 Nsk Ltd Rolling guide device
JP2014517151A (en) * 2011-05-17 2014-07-17 アクティエボラゲット・エスコーエッフ Improved bearing steel

Similar Documents

Publication Publication Date Title
WO2012053541A1 (en) Steel for cold forging/nitriding, steel material for cold forging/nitriding, and cold-forged/nitrided component
WO2010116555A1 (en) Steel for case hardening which has excellent cold workability and machinability and which exhibits excellent fatigue characteristics after carburizing and quenching, and process for production of same
WO2017122830A1 (en) Steel wire for non-thermal-refined machine component, and non-thermal-refined machine component
JP2005054227A (en) Low carbon free cutting steel
JP4267234B2 (en) Hot rolled steel for machine structure with excellent forgeability and machinability
JP6241136B2 (en) Case-hardened steel
JP2008088478A (en) Steel component for bearing having excellent fatigue property
JP2010516898A (en) Lead-free free-cutting steel and its use
JP6461672B2 (en) Bolt steel wire and bolt with excellent cold forgeability and delayed fracture resistance after quenching and tempering
JP4014042B2 (en) Induction hardening steel bar
JPH11279710A (en) Bearing steel excellent in acoustic property and quietness
JP3541844B1 (en) Hot-forged non-tempered steel bars
JP2003113448A (en) Steel for bearing superior in silent property
JPH02156045A (en) Steel for corrosion-resisting rolling parts and rolling parts
JP2841468B2 (en) Bearing steel for cold working
EP1669468A1 (en) Steel product for induction hardening, induction-hardened member using the same, and methods for producing them
JP6265048B2 (en) Case-hardened steel
JP2019218584A (en) bolt
WO2023105852A1 (en) Stainless steel having excellent cold forgeability, hydrogen embrittlement resistance properties or corrosion resistance and non-magnetism
JP7464821B2 (en) Steel for bearing raceways and bearing raceways
JP7135484B2 (en) Carburizing steel and parts
JP5423571B2 (en) Hot-worked high carbon steel for induction-hardened parts
JP2022170056A (en) steel
JP2017039971A (en) Case hardening steel for high strength cold forging
JP6172378B2 (en) Case-hardened steel wire

Legal Events

Date Code Title Description
A02 Decision of refusal

Effective date: 20040316

Free format text: JAPANESE INTERMEDIATE CODE: A02